二氯喹啉酸及其代谢物在稻田水土作物中的气谱和液谱残留分析方法研究

Residue Determination of Dichloroquinolinecarboxylic Acid and its Metabolite in Water, Soil and Rice Plant by GC and HPLC.

本文提供了二氯喹啉酸及其代谢物简便、快速、灵敏、准确的分析方法。稻田水和土壤样，不必净化和衍生直接用液谱测定，二氯喹啉酸的检测极限，在田水中为0．002mg／kg，在土壤中为0．005mg／kg；代谢物在土壤中为0．010mg／kg。土壤样亦可用C_3键合硅柱萃取、重氮化、气谱测定。二氯喹啉酸检测极限为0．001mg／kg，代谢物为0．005mg／kg。茎叶（稻秆）、稻壳、糙米样经提取、净化、重氮化，用气谱测定，二氯喹啉酸检测极限为0．005mg／kg。添加回收率均在80％以上。

The simple, rapid, sensitive and accurate methods for analysis of dichloroquinolinecarboxylic acid (Ⅰ) and its metabolite (Ⅱ) from water, soil and rice plant were developed. water and soil samples could be analyzed directly by HPLC without clean-up and derivatization. The detection limits for (Ⅰ) was 0.002 mg/kg in rice field water; 0.003mg/kg in soil; and for (Ⅱ) was 0.010 mg/kg in soil. Soil samples also could he extracted by C8 bonded phase silica. Gas chromatography of the resulting concentrate after methylation with diazomethane gave 0.001 mg/kg sensitivity for (Ⅰ) and 0.005 mg/kg for (Ⅱ). (Ⅰ) in and on rice leaves and rice straws; in rice husk; in unpolished rice can be determined by GC after extraction, cleanupand methylation with aidzomethane. The limits of 0.005 mg/kg for (Ⅰ)could be attained. HPLC and GC methods gave 82.8-100.3 for (Ⅰ) and 75.7-91.7% for (Ⅱ) recoveries.